First X-Ray Crystal Structure and Internal Reference Diffusion-Ordered NMR Spectroscopy Study of the Prototypical Posner Reagent, MeCu(SPh)Li(THF)3

2013 ◽  
Vol 19 (31) ◽  
pp. 10138-10141 ◽  
Author(s):  
Steven H. Bertz ◽  
Richard A. Hardin ◽  
Thomas J. Heavey ◽  
Daniel S. Jones ◽  
T. Blake Monroe ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Spectroscopy Study ◽  
Internal Reference ◽  
X Ray

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Nuclear magnetic resonance studies on the anions [M(SnCl3)5Cl]4− (M = Ru, Os) and [Ru(SnCl3)5(MeCN)]3−: the X-ray crystal structure of [N(C2H5)4]4[Ru(SnCl3)5Cl]

1982 ◽  
Vol 60 (11) ◽  
pp. 1304-1316 ◽  
Author(s):  
Louis J. Farrugia ◽  
Brian R. James ◽  
Claude R. Lassigne ◽  
Edward J. Wells
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Octahedral Geometry ◽  
Coupling Constants ◽  
Order Effects ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Crystallographic Study

The octahedral anions [M(SnCl3)5Cl]4− (M = Ru, Os) have been fully characterized by 119Sn FT nmr spectroscopy. For M = Ru, 117Sn and 115Sn nmr spectra were also recorded, and an X-ray crystallographic study was carried out on the tetraethylammonium salt, isolated as a disolvate from acetonitrile. The Ru—Sn bond lengths indicate some degree of dπ–dπ interactions. The slight distortions from octahedral geometry are discussed in connection with the packing of the chlorine atoms. The Sn nmr spectra reveal the first observed coupling to a 99Ru nucleus (I = 5/2, 12.7% natural abundance), very large 2J(119Sn—117Sn) coupling constants, and the first observed second-order effects on a heteronuclear system. The octahedral anion [Ru(SnCl3)5(MeCN)]3− was also synthesized as the tetraethylammonium salt and characterized spectroscopically.

A Domino Reaction for the Synthesis of Novel 1,3-Dihydrofuro[3,4-c]pyridines from Pyridoxal and Ketones

Synthesis ◽  
2020 ◽  
Vol 53 (02) ◽  
pp. 365-370
Author(s):  
Lucas Pizzuti ◽  
Izamara Casadia ◽  
Thalita O. Daher ◽  
Sidnei Moura ◽  
Davi F. Back ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
13C Nmr ◽  
Room Temperature ◽  
13C Nmr Spectroscopy ◽  
Domino Reaction ◽  
Alkyl Aryl ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Pyridine Series

A convenient domino route for the synthesis of novel 1,3-dihydrofuro[3,4-c]pyridines from pyridoxal and alkyl, aryl or heteroaryl ketones under basic conditions is reported. A series of nine derivatives is obtained in 53–90% yields after stirring reactants for 48 hours at room temperature. Most products are easily isolated by filtration followed by recrystallization from ethanol. All products were fully characterized by FTIR, HRMS, and 1H and 13C NMR spectroscopy. The X-ray crystal structure of a representative example of the 1,3-dihydrofuro[3,4-c]pyridine series is also presented.

Lanthanide Complexes with Carbacylamidophosphates: The First Registration of Chelate Coordination of the Neutral Ligand Form in the Structure of Di-(N,Nf-tetramethyl-NM -benzoylphosphoryl- triamide)cerium(III) Nitrate

2000 ◽  
Vol 55 (7) ◽  
pp. 576-582 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Helmut Fischer ◽  
Rüdiger Stumpf ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Coordination Compounds ◽  
Metal Ion ◽  
Lanthanide Complexes ◽  
Carbonyl Oxygen ◽  
Neutral Ligand ◽  
Crystal Data ◽  
X Ray

Abstract The coordination compounds of the general formula Ln(HL)2(NO3)3, (where Ln = La - Eu (without Pm), HL = C6H5C(O)NHP(O)[N(CH3)2]2, N,Nʹ-tetramethyl-Nʺ-benzovlphosphoryl-triamide) have been synthesized and characterized by means of IR, UV-VIS, 1H, 31P NMR spectroscopy, and X-ray analysis. The complexes are isostructural according to X-ray powder diffraction studies. The crystal structure of the cerium(lll) complex has been determined. Crystal data: monoclinic, P21/c, with a = 10.503(9), b = 15.62(2), c = 21.91(2) Å, β = 99.56(8)°, Z = 4, V = 3546(6) Å3, R1= 0.0550, wR2 = 0.1383 for 6970 unique reflections used. The complex has a molecular structure. Neutral phosphoryltriamide ligands are coordinated to the metal ion in a bidentate manner via phosphoryl and carbonyl oxygen atoms with formation of six membered chelate rings. The coordination polyhedron of the Ce atom is a sphenocorona; C.N. = 10 (4 O[HL] + 6 O [NO3-]).

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